本研究基于在线固相萃取-液相色谱-四极杆/静电场轨道阱高分辨质谱建立了同时测定牛奶中10种利尿剂的测定方法.试样采用乙腈提取,提取液经在线固相萃取柱净化,待测物在CAPCELL PAK ADME(150 mm×2.1 mm,5 µm)色谱柱上用乙腈-水进行梯度洗脱分离.同时,采用加热电喷雾电离源(Heat Electric Spray Ion Source,HESI)以正负离子全扫描/数据依赖二级扫描模式进行分析,外标法定量.结果显示,10种利尿剂在各自线性范围内线性关系良好,相关系数(r)大于 0.9978,检出限(LODs)为 1～3 µg/kg,定量限(LOQs)为 3～10 µg/kg,平均回收率在 73.6%～104.2%之间,相对标准偏差(RSDs)在 3.6%～8.1%之间.该方法操作简单、灵敏度高、准确性好,可为相关检测人员提供更高效的解决方案.
Rapid Determination of 10 Diuretics in Milk by on-Line Solid Phase Extraction Coupled with Liquid Chromatography-High Resolution Mass Spectrometry
A novel method was developed for the rapid determination of 10 diuretics in milk by on-line solid phase extraction coupled with liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry(Online-LC-Q/Orbitrap HRMS).The samples were extracted with acetonitrile,then purified by an on-line solid phase extraction column,and subsequently separated on an CAPCELL PAK ADME(150 mm×2.1 mm,5 µm)column using a gradient elution with acetonitrile-water as the mobile phase.The diuretics were analyzed employing a Heat Electric Spray Ion source(HESI)in both positive and negative ion Full Scan/ddMS2 modes,and quantification was performed using the external standard method.The results demonstrated excellent linearity within the tested concentration ranges,with correlation coefficients(r)greater than 0.9978.The limits of detection(LODs)ranged from 1-3 µg/kg,and the limits of quantitation(LOQs)from 3-10 µg/kg.The average recoveries for the 10 diuretics were between 73.6%and 104.2%,with relative standard deviations(RSDs)of 3.6%-8.1%.This method is straightforward to perform,highly sensitive,and accurate,offering a more efficient solution for detection personnel.
on-line solid phase extractionliquid chromatographyelectrostatic field obitrap high-resolution mass spectrometrydiureticsmilk
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